NIST Procedure For Method Validation 20180101
NIST Procedure For Method Validation 20180101
NIST Procedure For Method Validation 20180101
1. Introduction
This is the metrology laboratory policy and procedure for developing and validating test or
calibration methods when no international or national procedures are available, when
deviating from standardized methods, or when no standard procedures are available.
2. Purpose
The Metrology Laboratory follows this procedure to ensure that all laboratory methods selected,
modified, or developed for tests and calibrations are appropriate for the intended use, properly
documented, validated, accepted by laboratory management, and agreed upon by the client.
Customers of the Laboratory expect a given service to provide acceptable measurement results
when they request a test or calibration. The laboratory must evaluate each method to ensure that
it has qualified and competent staff, suitable facilities, equipment, and standards with acceptable
metrological traceability to perform the test or calibration.
3. Responsibility
3.2. The Technical Manager reviews the documented procedure, data, and analysis, and
recommends final acceptance to the Laboratory Manager or Quality Manager based on
the suitability of the procedure and acceptability of observed analysis of measurement
results.
3.3. The Laboratory Supervisor or Quality Manager is responsible for final acceptance of
new calibration methods, training staff on the new procedure, and for consistent
implementation.
4. Operations
4.1.If the laboratory does not have an appropriate method for a calibration or test, or the test
or calibration requires deviation to meet the needs of the customer, the Technical
Manager is notified and this procedure is implemented.
4.2. When determining whether to proceed in developing new test or calibration method to
meet the needs of a customer, the Laboratory Supervisor or Quality Manager and
4.3. The staff conducting the Contract Review for the calibration or test must obtain a clear
specification of the customer requirements and the purpose of the test or calibration
including any tolerances or maximum uncertainties that are required for the item/sample
end usage (to ensure that the measurement results will be fit for purpose).
4.4. New methods must be developed prior to performing the tests or calibrations and contain
the following information:
4.4.1. appropriate identification (title);
4.4.2. scope or range of test;
4.4.3. description of the type of item to be tested or calibrated;
4.4.4. parameters or quantities and ranges to be determined;
4.4.5. apparatus and equipment, including technical performance requirements;
4.4.6. reference standards and reference materials required;
4.4.7. environmental conditions required and any stabilization period needed;
4.4.8. description of the procedure, including any special items as noted in this list:
4.4.8.1. affixing of identification marks, handling, transporting, storing and
preparation of items,
4.4.8.2. checks to be made before the work is started,
4.4.8.3. checks that the equipment is working properly and, where required,
calibration and adjustment of the equipment before each use,
4.4.8.4. the method of recording the observations, data to be recorded, data
reduction, method of analysis, and presentation of results, and
4.4.8.5. any safety measures to be observed;
4.4.9. criteria and/or requirements for approval/rejection where applicable;
4.4.10. data to be recorded and method of analysis and presentation; and
4.4.11. the uncertainty or the procedure for estimating uncertainty.
5. Method Validation
5.2. Validation methods are to be as extensive as necessary to meet the needs of their
intended application. Adequate measurement data is obtained to ensure statistical
validity of the evaluated results. The accuracy and uncertainty of test or calibration
results shall be assessed for the intended use, and shall be relevant to the client’s needs.
5.5. When changes are made in the validated non-standardized procedures, the influence of
such changes must be documented and, if appropriate, a new validation process carried
out.
5.6. The following types of assessments, with data and statistical analysis are examples that
may be used to assess the measurement results (See Appendix A form):
5.6.1. Inspection and technical assessment of the essential elements of metrological
traceability to ensure presence and adequacy (technical review may include
representatives from other laboratories, working groups, technical experts, and
assessors):
5.6.1.1. Reference to the international system of units (SI);
5.6.1.2. Unbroken chain of calibrations to national and/or international standards;
5.6.1.3. Suitable and up to date calibration intervals for standards used in the
procedure;
5.6.1.4. Documented procedure (reviewed to ensure completeness against the list
of items in Section 4.d.);
5.6.1.5. Documented measurement uncertainty (as noted in Section 4.d.v.);
5.6.1.6. Demonstrated technical competence;
5.6.1.7. Adequate measurement assurance approach and supporting data.
5.6.2. Accuracy or Limits to Bias may use data obtained from internal testing and/or
interlaboratory comparisons: t-test, normalized error (En), absolute or relative bias
versus required tolerance limits;
5.6.3. Precision: standard deviation, normalized precision (Pn), F-test, comparison to
required uncertainties (fit for purpose and meeting needs of the customer)
5.6.4. Repeatability: assessment of results over time and by different operators
following the procedure as documented
5.6.5. Reproducibility: assessment of data from other laboratories following the
procedure
6. Records (See Appendix A for minimum summary to be supplemented with appropriate data,
analysis, and evaluation records).
7. Implementation
This procedure has found to be complete, fit for its intended use, technically validated, meets customer needs,
and is approved for use.
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